FORMULATION & EVALUATION OF SHAMPOO

V.MANIMARANLECTURERDEPARTMENT OF PHARMACEUTICSSRM COLLEGE OF PHARMACY

UNIT V

CONTENTS

1. Introduction

2. Types of Shampoos

3. Product Ingredients

4. Formulation

5. Evaluation of Shampoos

6. References

Introduction• Definition: A shampoo is a preparation of a surfactant (i.e.

surface active material) in a suitable form – liquid, solid orpowder – which when used under the specified conditionswill remove surface grease, dirt, and skin debris from the hairshaft and scalp without adversely affecting the user.

• Requirements of a Shampoo:1. It should effectively and completely remove dust or soil,

excessive sebum or other fatty substances and loose cornealcells from the hair.

2. It should produce a good amount of foam to satisfy thepsychological requirements of the user.

3. It should be easily removed on rinsing with water.4. It should leave the hair non‐dry, soft, lustrous with good

manageability and minimum fly away.5. It should impart a pleasant fragnance to the hair.6. It should not cause any side‐effects / irritation to skin or eye.7. It should not make the hand rough and chapped.

Types of Shampoo

Shampoos are of the following types:Powder ShampooLiquid ShampooLotion ShampooCream ShampooJelly ShampooAerosol ShampooSpecialized Shampoo

• Conditioning Shampoo• Anti‐ dandruff Shampoo• Baby Shampoo• Two Layer Shampoo

PRODUCT INGREDIENTS• Surfactants are the main component of shampoo. Mainly anionic

surfactants are used.

• The raw materials used in the manufacture of shampoos are:

1. Principal surfactants: Provide detergency and foam.

2. Secondary surfactants: Improve detergency, foam and haircondition.

3. Other additives.

CLEANSING ACTION OF SHAMPOOA surfactant consists of two part‐ one hydrophilic (water loving) 

while the other is hydrophobic in nature.

Surfactants

Anionic surfactants are mostly used (good foamingproperties). The hydrophilic portion carries a negativecharge which results in superior foaming, cleaningand end result attributes.Non‐ionic surfactants have good cleansing properties but do not have sufficient foaming power.Cationic surfactants are toxic and are hence not used. However, they may be used in low concentration in hair conditioners.Ampholytics, being expensive, are generally not used. However, they are mainly used as secondary surfactants and good hairconditioners.

ANIONIC SURFACTANTSCLASS EXAMPLE COMMENT

Alkyl benzene sulfonates

Sodium dodecyl benzene sulfonate

Tend to yield an “airy” or low density foam and often are drying to the hair

Primary alkyl sulfates Lauric acid, stearic acid andtheir salts

Good lathering effect in hard water, free from rancidity, easy to wash.

Secondary alcohol sulfates

Sodium sec‐lauryl sulfate Low cost, dispersing and emulsifying action, dissapointing as detergets and shampoo components

Alkyl benzene polyoxyethylenesulfonates

Triton X200 Stable in acid or alkaline solution, excellent emulsifier, detergent and wetting agent; extremely stable at pH of skin

Sulfated monoglycerides

Lauric monoglycerideammonium sulfate

Stable in hard water

Alkyl ether sulfates Derivatives of lauryl alcohol ether with PEG

Good cleansers, act as solvents for non polar additives

Sarcosines Lauroyl and cocoylsarcosines

Excellent foaming and conditioning action

Sulfosuccinates Aerosol OT Less irritating to skin and eye (baby shampoo)

Maypon Protalbinic and lysalbinicacid derivatives (maypon 4C)

Hydrolysation product of proteins with fatty acid chlorides in presence of alkali

NON‐IONIC SURFACTANTS

CLASS EXAMPLE COMMENTS

Fatty acid alkanolamides (should not be used > 15%)

Lauric monoethanolamide Improves solubility of SLS

Stearic ethanolamide Pearlescent thickener

Oleic ethanolamides Hair conditioning agents

Polyalkoxylatedderivatives

Ethoxylated fatty alcohols Stable in wide range of pH; stabilizing emulsifying and opacifying properties

Block polymers (pluronics) Good rinsability, can be used in high %

Sorbitol esters (TWEENS) Solubilizers and emulsifiers, used in baby shampoos

Amine oxides Coconut and dodecyldimethyl amine oxides

Foam booster and anti‐static agents

AMPHOTERIC SURFACTANTS

N‐alkyl aminoacids β – aminoacid derivatives Foaming agents

Aspargine derivatives Compatible with both anionic and cationic surfactants

Betains Amido betains High foaming properties, mild.

Alkyl imidazoline MIRANOLTM Baby shampoos

ADDITIVESConditioning agents: Lanolin, mineral oil, herbal extracts, egg derivatives.Foam builders: Lauroyl monoethanolamide, sarcosinatesViscosity modifiers : 

Electrolytes – NH4Cl, NaClNatural gums – Gum Karaya, tragacanth, alginatesCellulose derivatives – Hydroxy ethyl cellulose, methyl celluloseCarboxy vinyl polymers – Carbopol 934 Others – PVP, phosphate esters.

Sequestering agents : EDTAOpacifying agents : Alkanolamides of higher fatty acids, propylene glycol, Mg, Ca and Zn salts of stearic acid, spermaceti, etc.Clarifying agents : 

Solubilizing alcohols – ethanol, isopropanolPhosphates –Non‐ionic solubilizers – polyethoxyated alcohols and esters.

ADDITIVES

Perfumes : Herbal, fruity or floral fragnances.

Preservatives : Methyl and propyl paraben, formaldehyde (most effective).

Anti‐dandruff agents: The shampoos contain smallamount of these actives, which are in contact withthe scalp for only a short time. In order to beeffective the active ingredient must work in the oil‐water environment of the scalp and must be readilysubstantive to the scalp for continuing activity.

Ex: Selenium sulfide, zinc pyrithone, salicylic acid.

FORMULATIONS

POWDER SHAMPOOHenna powder 5%

Soap powder 50%

Sodium carbonate 22.5%

Potassium carbonate 7.5%

Borax 15%

Perfume q.S

LIQUID SHAMPOOSLS 40%

NaCl (to desired viscosity) 2‐4%

Water Upto 100%

Perfume, color, preservatives q.s

LOTION SHAMPOOTLS 35%

Glyceryl monostearate 2%

Magnesium stearate 1%

Water Upto 100%

Color q.s

Perfume, preservatives q.s

FORMULATIONS

CREAM SHAMPOOSLS 38%

Cetyl alcohol 7%

Water Upto 100%

Color, perfume q.S

Preservative q.s

JELLY SHAMPOOSAlkyl dimethyl benzalkonium chloride 15%

TLS (40%) 28%

Coconut ditethanolamide 7%

HPMC 1%

Water  Upto 100%

Color, perfume, preservative q.s

AEROSOL SHAMPOOTLS 60%

Coconut diethanolamide 2%

Water Upto 90%

Propellent 10%

Color, perfume, preservative q,.s

FORMULATIONS

CONDITIONING SHAMPOOSSteryl dimethyl benzyl ammonium chloride

5.5%

Ethylene glycol monostearate

2%

Cetyl alcohol 2.5%

Water Upto 100%

Color, perfume, preservative q.s

TWO LAYER SHAMPOO

SLS 27%

Cocamidopropylamine oxide 5%

Lauramine DEA 1%

Lactic acid (50%) 1%

Formaldehyde 0.1%

BABY SHAMPOO

Magnesium lauryl sulfate (27.5%) 11%

Cocamidopropyl betaine (30%) 5%

Polysorbate 20 1%

PEG 600 3.5%

Perfume q.S

Preservative q.S

Citric acid To pH 6

Color q.S

Water (deionised); Aqua (INCI) To 100%

FORMULATIONS

ANTI‐DANDRUFF SHAMPOOThymol 0.05%

Menthol 0.1%

Camphor 0.1%

TLS 55%

Water upto 100

Color, perfume, preservative q.s

ANTI‐DANDRUFF SHAMPOO

Selenium sulfide 2.5%

Bentonite 5%

SLS paste 35%

Water upto 100

Color, perfume, preservative q.s

FORMULATIONHERBAL SHAMPOO

Natural essential oil blend 0.5%

Cyamopsis tetragonoloba (Guar Gum) 1%

Camellia sinensis (Green Tea) extract 2%

Glycerin 1%

Hydrolysed wheat protein 2.5%

Salvia officinalis (Sage) leaf extract 1.5%

Salvia officinalis (Sage) 1.5%

Glyceryl oleate 1%

Polysorbate 20 0.5%

Potassium sorbate 5%

Aloe barbadensis (Aloe vera) extract 0.5%

Arctium minus (Burdock) root extract 0.5%

Disodium coco‐glucoside sulfosuccinate 0.5%

Preservatives q.s.

Water Upto 100%

Evaluation of ShampoosPerformance characteristics

Foam and foam stabilityDetergency and cleaning action

Effect of water hardnessSurface Tension and wettingSurfactant content and analysis

RinsingConditioning action

SoftnessLusterLubricityBody, texture and set retentionIrritation and toxicityDandruff control

Microbiological assayEye irritancy test

Product characteristicsFragnanceColourConsistencyPackage

1. Foam and foam stability:• The Ross‐Miles foam column test is accepted. 200 ml of surfactant

solution is dropped into a glass column containing 50ml of the samesolution. The height of the foam generated is measured immediatelyand again after a specified time interval, and is considered proportionalto the volume.

• Barnett and Powers developed a latherometer to measure the effect ofvariables such as water hardness, type of soil and quantity of soil onfoam speed, volume and stability.

• Fredell and Read titrated actual standard oiled heads of hair withadditive increments of shampoo until a persistent lather end pointappeared.

2. Detergency and cleaning action:• Cleansing power is evaluated by the method of Barnet and Powers• 5gm sample of soiled human hair is placed at 35°c in 200 cc of water

containing of 1 gm of shampoo.• The flask is shaken 50 times a minute for 4 minutes. Then washed once

again with sufficient amount of water, then after filter the hair driedand weighed.

• The amount of soil is removed under these condition is calculated.

3. Wetting Action:• Canvas disk sinking test: A mount veron cotton duck # 6 canvas disk 1

inch in diameter, is floated on the surface of a solution, and the timerequired for it to sink is measured accurately.

4. Rinsing:• Skilled beauticians are employed to make comparisons on the

performance of several shampoos.

5. Conditioning Action:• Conditioning action is a difficult property to assess. This is because it is

basically dependent on subjective appraisal.• No method has been published for measuring conditioning action.• The degree of conditioning given to hair is ultimately judged by

shampoo user who is making the evaluation on the basis of pastexperience and present expectations.

6. Microbiological assay:PREPARATION OF PRE‐INOCULUM Take the loopful culture ofstaphylococcus aureus (ATCC6532) aseptically and transfer tosterilized and cooled 100 ml SCDM (broth).

• Mix well. Incubate the broth at 37oC for 24 hrs.PREPARATION OF MEDIA Soya bean casein digests medium, soyabean casein digest agar and nutrient agar.PREPARATION OF POUR PLATES Sterilized SCD agar (100 ml) iscooled to 40°C and mixed with 5 ml of 24 hrs old pre inoculatedculture.

• This is immediately poured in plates (340 ml each) and allows toset.MAKING THE WELLS ON AGAR PLATES The wells are dig on agarplates with sterilised well digger aseptically.

• Take 100µml of each sample, add to well aseptically. Incubate theplates at 37oC for 24 hrs to 48 hrs.

• Observe the effectiveness of sample on culture growing on the agarplate and we can see the effectiveness of sample in the form ofzone of inhibition around each well containing different sample.

7. Evaluation of eye irritancy:• The test calls for dropping 0.1 ml of liquid shampoo in the 

conjunctiva sac of one eye of the rabbit , the other eye serving as control. 

• In the case of the first three animals, the treated eye remains unwashed. Since washing the eye may or may not alleviate symptoms of injury. 

• The six remaining animals are divided into two equal groups. • In the first of these groups eyes instilled with the substances are 

washed with 20 ml of lukewarm water two seconds after treatment and in the second group after instillation. 

• Readings are then made at 24, 48 and 72 hr and again four and seven days after treatment. 

• If the lesions have not cleared up in seven days the test material is considered as severe irritant. 

8. Viscosity:• Viscosity of the liquid shampoo is determined using a Brookefield

viscometer• 100 mL of the shampoo is taken in a beaker and the spindle is 

dipped in it for about 5 min and then the reading is taken. 

References1. Balsam, S.M., Gershon, S.D., Rieger, M.M., Sagarin, E., and Strianse, S.J.: COSMETICS–

Science and Technology, 2nd edition, Vol‐2, John Wiley India, New Delhi, 2008

2. Barel, A.O., Paye, M., and Maibach, H.I.: Handbook of Cosmetic Science andTechnology, 3rd Edition, Informa Healthcare, New York.

3. Sharma, P.P.: COSMETICS ‐ Formulation, Manufacturing and Quality Control, 4th

Edition, Vandana Publishers Pvt. Ltd., New Delhi, March 1998.

4. Butler, H.: POUCHER’S – Perfumes, Cosmetics & Soaps, 10th Edition, Springer,Cockermouth, Cumbria, USA, 2000.

5. Salador, A., and Chisvert, A.: Analysis of cosmetic products, Elsevier, New York, 2006.

6. Ross, J., and Miles, G.D.: An application for comparison of foaming properties ofsoaps and detergents, Oil and Soap, 1941.

7. Mittal,: A Handbook of Cosmetics

8. Fredell, W.G., and Powers, D.H.: Factors attributing to the performance of shampoosand to consumer acceptance, Proc. Sci. Sec., 1955.

9. Rajkumar, K. J., Invitro evaluation of shampoos.

10. www.cosmeticdatabase.com